Patent RU-2623070-C1 (RU)
Inventor: SHORMANOV VLADIMIR KAMBULATOVICH
IPC: G01N33/52
Filed: 2016-04-20
Granted: 2017-06-21
Abstract: FIELD: chemistry. 
     SUBSTANCE: invention relates to a method for the determination of O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methylcarbamate and O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-(dibutylaminosulphenyl)-N-methylcarbamate in a biological material. The essence of the method is that a biological object containing O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methylcarbamate or O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-(dibutylaminosulphenyl)-N-methylcarbamate, ground, three times treated with a mixture of acetone and ethyl acetate, taken in a ratio of 6:4 by volume, each time for 30 minutes. The extracts obtained are combined, the extractant is evaporated, the residue is repeatedly treated with acetone. The acetone extracts are separated, combined, the solvent from the combined recovery is evaporated, the residue is dissolved in acetonitrile. The resulting solution is diluted with water in a ratio of 1:4 by volume, the resulting aqueous-acetonitrile solution is saturated with sodium chloride. Then it is extracted twice with ethyl acetate, the organic extracts are combined and evaporated to dryness. The residue is dissolved in acetone, introduced into a sorbent macrocolumn, which is silica gel KSS No 3 80/120 mcm. The chromatography is carried out using a two-component mobile phase of hexane-dioxane in a ratio of 8:2 by volume. The eluate fractions containing the analyte are combined, the eluent is evaporated, the residue is dissolved in methanol. Next, the test substance is determined by the chromatography-mass spectrometric method in a HP-5MS capillary column 30 m and inner diameter 0.2 mm with a stationary phase (5% -phenyl-95% -methyl polysiloxane, with a fixed film thickness of 0.25 mcm) using a helium carrier gas fed at a rate of 1.0 ml/min and a mass selective detector operating in the electron impact, where the initial temperature of the column thermostat is 70°C, this temperature is maintained for 2 minutes, further the temperature rises from 70 to 200°C a speed of 40°C per minute, and then 200 to 290°C with a speed of 12.5°C, the final column temperature is maintained for 2 minutes, the injector temperature is 250°C, the temperature of the quadrupole 150°C, the interface temperature of the detector 290°C, the intensity of the signal due to the charged particles formed during bombardment of the analyte that emerged from the capillary column and got to the ion source by an ionizing electron beam with an energy of 70 eV is recorded. The mass spectrum is recorded in terms of the total ion current and the amount of the aliphatic substance being O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methylcarbamate or O-(2,3-digin-2,2-dimethyl-7-benzofuranyl)-N-(dibutylaminosulphenyl)-N-methylcarbamate, by the area of the chromatographic peak. Using the method, O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl)-N-methylcarbamate and O-(2,3-dihydro-2,2-dimethyl-7-benzofuranyl) can be determined with high accuracy -N-(dibutylaminosulphenyl)-N-methylcarbamate in a biological material. 
     EFFECT: increased accuracy of determination. 
     4 tbl, 3 ex